CN114854487A - Extraction process for improving effective medicinal value components of camellia oil - Google Patents
Extraction process for improving effective medicinal value components of camellia oil Download PDFInfo
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- CN114854487A CN114854487A CN202210581856.7A CN202210581856A CN114854487A CN 114854487 A CN114854487 A CN 114854487A CN 202210581856 A CN202210581856 A CN 202210581856A CN 114854487 A CN114854487 A CN 114854487A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/02—Pretreatment
- C11B1/04—Pretreatment of vegetable raw material
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B1/00—Production of fats or fatty oils from raw materials
- C11B1/10—Production of fats or fatty oils from raw materials by extracting
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/006—Refining fats or fatty oils by extraction
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/10—Refining fats or fatty oils by adsorption
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B3/00—Refining fats or fatty oils
- C11B3/12—Refining fats or fatty oils by distillation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Microbiology (AREA)
- Fats And Perfumes (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses an extraction process for improving effective medicinal value components of camellia oil, which comprises the following steps: s1, cleaning and removing impurities from the camellia seeds, drying, shelling, separating shells and kernels, crushing and sieving to obtain camellia seed kernel powder; s2, performing reflux extraction on the camellia seed kernel powder by using ethanol as a solvent, and collecting camellia seed sediment and a camellia oil extracting solution obtained after reflux extraction; s3, adding water and sodium chloride into the tea seed sediment, adjusting the pH value with glacial acetic acid, adding enzyme for extraction, wherein the enzyme comprises protease and cellulase, standing for layering, and taking an upper oil layer to obtain crude oil; s4, stepThe crude oil obtained in step S3 is passed through supercritical CO 2 Extracting, and collecting the extracted tea oil; the camellia oil obtained by the method has high medicinal value and high oil yield.
Description
Technical Field
The invention relates to the field of camellia oil extraction, and in particular relates to an extraction process for improving effective medicinal value components of camellia oil.
Background
The Camellia oil is obtained from seeds of Camellia oleifera (Camellia oleifera abel) trees in the family of Camellia, is one of the oldest woody edible plant oils in China, is the country with the widest distribution of Camellia plants in the world, and is the largest tea oil production base in the world. The central production places of the oil tea are distributed in the Dabie mountain region, southwest, Hunan, Gannan and Jiangxi west of China, and are the unique oil tree species in China, which is the original production place of the oil tea. The oil tea tree grows in a non-polluted subtropical south-green humid climate area, and no pesticide, chemical fertilizer and the like are applied in the whole growth process. The latitude and longitude and the soil climate are suitable for the soil and have high nutrient content. Does not contain harmful substances to human body such as erucic acid, cholesterol, aflatoxin and the like. Golden or light yellow color, pure quality, clarity, transparency, fragrant smell and pure taste.
The camellia oil is rich in various lipid accompaniments besides high oleic acid, wherein the content of phenolic compounds is high, and the camellia oil has multiple effects of oxidation resistance, inflammation resistance and the like; how to ensure the good quality and the high oil yield of the camellia oil is very important.
Disclosure of Invention
The invention aims to provide an extraction process for improving effective medicinal value components of camellia oil, which aims to solve the problems of ensuring good quality and high oil yield of the camellia oil, and in order to realize the aim, the invention provides the following technical scheme:
an extraction process for improving effective medicinal value components of camellia oil comprises the following steps:
s1, cleaning and removing impurities from the camellia seeds, drying, shelling, separating shells and kernels, crushing and sieving to obtain camellia seed kernel powder;
s2, performing reflux extraction on the camellia seed kernel powder by using ethanol as a solvent, and collecting camellia seed sediment and a camellia oil extracting solution obtained after reflux extraction;
s3, adding water and sodium chloride into the tea seed sediment, adjusting the pH value with glacial acetic acid, adding enzyme for extraction, wherein the enzyme comprises protease and cellulase, standing for layering, and taking an upper oil layer to obtain crude oil;
s4, processing the crude oil obtained in the step S3 by supercritical CO 2 Extracting, and collecting the extracted tea oil;
s5, decoloring and deodorizing the extracted camellia oil obtained in the step S4 to obtain decolored and deodorized camellia oil;
s6, distilling off ethanol from the camellia oil extract obtained in the step S2, adding petroleum ether with the same volume for extraction, separating an ether phase and a water phase after layering, repeating the extraction process on the obtained water phase for 3-4 times, mixing the obtained ether phases, distilling off the petroleum ether, retaining the water phase to obtain a camellia oil extract, drying the camellia oil extract, and adding the dried camellia oil extract into the decolored and deodorized camellia oil obtained in the step S5 for mixing to obtain a finished camellia oil product.
Preferably, in step S2: the reflux extraction specifically comprises the following steps: soaking the camellia seed kernel powder in 50% ethanol solution prepared from calcium hydroxide solution with pH of 9 for no less than 12 h; and carrying out reflux extraction after soaking for three times.
Preferably, in step S3: the mass ratio of the protease to the cellulase is 1: 1, the mass ratio of the tea seed precipitate, the water, the sodium chloride and the enzyme is 1:6:0.05:0.03, and the pH value is 5.
Preferably, the decoloring in step S5 is specifically: sucking the washed tea oil into a decolorizing tank, heating to 130 deg.C for dehydration for 20-30min, and reducing water content to below 0.1%; cooling to 110 deg.C, adding clay 5-7 wt%, decolorizing for 20min at vacuum degree of 97-99kPa, cooling to below 80 deg.C, and filtering to obtain decolorized tea oil.
Preferably, in step S5, the deodorization is specifically: sucking the decolored oil into a deodorization pot, heating to 110 ℃ by using indirect steam, heating to 150 ℃ by using heat conduction oil, turning over by using direct steam, heating to 245 ℃ at the speed of 4-5 ℃/min, preserving the heat for 1-1.2 hours, cooling the oil in the pot to 180-200 ℃ by using water at the temperature of 98-100 ℃, closing the direct steam, introducing cooling water into a steam pipe for cooling, cooling to 25 ℃, turning over, and repeating the steps for 2-3 times to obtain the deodorized tea oil.
Preferably, after adding petroleum ether with the same volume, stirring for 6-10min, standing for 10-15min, and repeating the stirring-standing process for layering.
Preferably, the camellia oil extract in step S6 includes camellia oil polyphenols.
Preferably, the camellia seeds are safflower camellia seeds.
Advantageous effects
In the invention, the camellia seeds are subjected to reflux extraction firstly, the camellia seed extract is separated out, the camellia seeds are subjected to aqueous enzymatic method firstly to prepare crude oil, and then supercritical CO is used 2 The extraction is carried out, the oil yield of the oil prepared by the aqueous enzymatic method is greatly improved compared with that of the oil prepared by the squeezing method, and the quality of the oil is ensured by the extraction; then, the tea seed extract is processed to obtain tea seed polyphenol compounds containing substances such as tea polyphenol, and the like, and the tea seed polyphenol compounds are added into the tea oil, so that the problem of how to ensure the oil quality of the camellia oil while improving the oil yield is solved, and the tea oil is endowed with better medicinal value.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in the embodiments of the present invention, and it is obvious that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
The camellia oil extraction process comprises the following steps:
s1, cleaning and removing impurities from the camellia seeds, drying, shelling, separating shells and kernels, crushing and sieving to obtain camellia seed kernel powder;
s2, 100g of camellia seed kernel powder is taken for reflux extraction, ethanol is adopted as a solvent, and the camellia seed sediment and the camellia oil extract obtained after reflux extraction are collected, wherein the reflux extraction specifically comprises the following steps: soaking the camellia seed kernel powder in 50% ethanol solution prepared from calcium hydroxide solution with pH of 9 for no less than 12 h; carrying out reflux extraction after soaking for three times, and drying the tea seed precipitate for later use;
s3, adding water and sodium chloride into the tea seed sediment, adjusting the pH value with glacial acetic acid, adding enzymes, and extracting, wherein the enzymes comprise protease and cellulase, and the mass ratio of the protease to the cellulase is 1: 1, standing and layering the tea seed sediment, water, sodium chloride and enzyme at a mass ratio of 1:6:0.05:0.03 and a pH value of 5, taking an upper oil layer to obtain crude oil, and weighing 27.3g of the crude oil;
s4, performing supercritical CO extraction on the crude oil obtained in the step S3 by using a supercritical extraction agent 2 Extracting, supercritical CO 2 Collecting the extracted tea oil under the conditions of 15MPa of pressure and 40 ℃ in the device;
s5, decoloring and deodorizing the extracted camellia oil obtained in the step S4 to obtain decolored and deodorized camellia oil;
the decolorizing and deodorizing steps comprise sucking washed tea oil into decolorizing tank, heating to 130 deg.C for dewatering for 20-30min to reduce water content to below 0.1%; cooling to 110 deg.C, adding clay 5-7 wt%, decolorizing for 20min at vacuum degree of 97-99kPa, cooling to below 80 deg.C, and filtering to obtain decolorized oleum Camelliae, wherein the deodorization is specifically: sucking the decolorized tea oil into a deodorization pot, heating to 110 ℃ by using indirect steam, heating to 150 ℃ by using heat conduction oil, turning over by using direct steam, heating to 245 ℃ at the speed of 4-5 ℃/min, preserving the heat for 1-1.2 hours, cooling the oil in the pot to 180-200 ℃ by using water at the temperature of 98-100 ℃, closing the direct steam, introducing cooling water into a steam pipe for cooling, cooling to 25 ℃, turning over, and repeating the steps for 2-3 times to obtain the deodorized tea oil;
s6, distilling the camellia oil extract obtained in the step S2 to remove ethanol, adding petroleum ether with the same volume to extract, separating an ether phase and a water phase after layering, repeating the extraction process on the obtained water phase for 3-4 times, mixing the obtained ether phases to remove the petroleum ether, keeping the water phase to obtain a camellia oil extract and a camellia oil extract, drying the camellia oil extract, adding the dried camellia oil extract into decolored and deodorized camellia oil to mix to obtain a finished camellia oil product, wherein the weight of the dried camellia oil extract is 5.1mg, detecting the camellia oil extract, the weight of total polyphenols of the camellia oil extract is 4.2mg, and weighing the finished camellia oil product by 25.9 g.
Comparative example 1
The camellia oil extraction process comprises the following steps:
s1, cleaning and removing impurities from the camellia seeds, drying, shelling, separating shells and kernels, crushing and sieving to obtain camellia seed kernel powder;
s2, adding water and sodium chloride into 100g of camellia seed kernel powder, adjusting the pH value with glacial acetic acid, adding enzyme, and extracting, wherein the enzyme comprises protease and cellulase, and the mass ratio of the protease to the cellulase is 1: 1, standing and layering the tea seed sediment, water, sodium chloride and enzyme at a mass ratio of 1:6:0.05:0.03 and a pH value of 5, taking an upper oil layer to obtain crude oil, and weighing the crude oil to obtain 27.6g of crude oil;
s3, performing supercritical CO extraction on the crude oil obtained in the step S3 by using a supercritical extraction agent 2 Extracting, and collecting the extracted tea oil;
s4, decoloring and deodorizing the extracted tea oil obtained in the step S4 to obtain a finished camellia oil product, wherein 26.1g of the finished camellia oil product contains 0.09 per mill of total polyphenol, about 2.34mg of total polyphenol in the finished camellia oil product.
Comparative example 2
Cleaning oil tea seeds, removing impurities, drying, husking, separating shells and kernels, crushing and sieving to obtain oil tea seed kernel powder; taking 100g of camellia seed kernel powder, carrying out physical squeezing to obtain 15.7g of crude oil, and detecting the total polyphenol content of the crude oil, wherein the total polyphenol content accounts for 0.17 per mill of the crude oil and is about 2.66 mg.
From the comparison between example 1 and comparative example 2, it can be seen that the yield of oil extracted by the aqueous enzymatic method is significantly higher than that of the conventional physical pressing, 100g of treated camellia seeds can be obtained by the aqueous enzymatic method, while the comparative example 2 only has 15.7g, and the comparison between example 1 and comparative example 1 shows that there is no difference in yield, i.e. the reflux extraction step has no influence on the oil extracted, whereas in terms of the content of polyphenols, the comparative example 1 is significantly lower than that of example 1, and the amount of camellia seeds in example 1 is 100g, so that 25.9g of polyphenols, 4.2mg, about 0.16%, and substantially identical to that of the physical pressing are obtained, while the polyphenols in comparative example 1 only account for 0.09% and about 2.34% of camellia oil, and the polyphenols in camellia oil contain tea polyphenols, so that the tea oil has better medicinal value.
Finally, it should be noted that: the above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (8)
1. An extraction process for improving effective medicinal value components of camellia oil is characterized by comprising the following steps:
s1, cleaning and removing impurities from the camellia seeds, drying, shelling, separating shells and kernels, crushing and sieving to obtain camellia seed kernel powder;
s2, performing reflux extraction on the camellia seed kernel powder by using ethanol as a solvent, collecting camellia seed precipitates obtained after reflux extraction, and obtaining a camellia oil extracting solution;
s3, adding water and sodium chloride into the tea seed sediment, adjusting the pH value to weak acidity by glacial acetic acid, adding enzymes including protease and cellulase, standing for layering, and taking the upper oil layer to obtain crude oil;
s4, processing the crude oil obtained in the step S3 by supercritical CO 2 Extracting, and collecting the extracted tea oil;
s5, decoloring and deodorizing the extracted camellia oil obtained in the step S4 to obtain decolored and deodorized camellia oil;
s6, distilling off ethanol from the camellia oil extract obtained in the step S2, adding petroleum ether with the same volume for extraction, separating an ether phase and a water phase after layering, repeating the extraction process on the obtained water phase for 3-4 times, mixing the obtained ether phases, distilling off the petroleum ether, retaining the water phase to obtain a camellia oil extract, drying the camellia oil extract, and adding the dried camellia oil extract into the decolored and deodorized camellia oil obtained in the step 5 for mixing to obtain a finished camellia oil product.
2. The extraction process according to claim 1, wherein in step S2: the reflux extraction specifically comprises the following steps: soaking the camellia seed kernel powder in 50% ethanol solution prepared from calcium hydroxide solution with pH of 9 for no less than 12 h; and carrying out reflux extraction after soaking for three times.
3. The extraction process according to claim 1, wherein in step S3: the mass ratio of the protease to the cellulase is 1: 1, the mass ratio of the tea seed precipitate, the water, the sodium chloride and the enzyme is 1:6:0.05:0.03, and the pH value is 5.
4. The extraction process according to claim 1, wherein the decoloring in the step S5 is specifically: sucking the washed tea oil into a decolorizing tank, heating to 130 deg.C for dehydrating for 20-30min until the water content is reduced to below 0.1%; cooling to 110 deg.C, adding clay 5-7 wt%, decolorizing for 20min at vacuum degree of 97-99kPa, cooling to below 80 deg.C, and filtering to obtain decolorized oleum Camelliae.
5. The extraction process according to claim 1, wherein in step S5, the deodorization is specifically: sucking the decolored oil into a deodorization pot, heating to 110 ℃ by using indirect steam, heating to 150 ℃ by using heat conduction oil, turning over by using direct steam, heating to 245 ℃ at the speed of 4-5 ℃/min, preserving the heat for 1-1.2 hours, cooling the oil in the pot to 180-200 ℃ by using water at the temperature of 98-100 ℃, closing the direct steam, introducing cooling water into a steam pipe for cooling, cooling to 25 ℃, turning over, and repeating the steps for 2-3 times to obtain the deodorized tea oil.
6. The extraction process according to claim 1, wherein step S6:
adding petroleum ether with the same volume, stirring for 6-10min, standing for 10-15min, and repeating the stirring-standing process for layering.
7. The extraction process according to claim 1, wherein the camellia oil extract in step S6 comprises camellia oil polyphenols.
8. The extraction process according to claim 1, wherein the camellia seeds are camellia safflower seeds.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232669A (en) * | 2022-08-11 | 2022-10-25 | 贵州山茶产业综合开发有限公司 | Preparation method of squalene-containing tea oil |
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| CN105567420A (en) * | 2015-12-24 | 2016-05-11 | 福建优创油脂有限公司 | Preparation method of health care tea oil |
| CN106190524A (en) * | 2016-08-18 | 2016-12-07 | 贵州石阡佛顶山野生油茶油业有限公司 | A kind of production method of aqueous enzymatic extraction Oleum Camelliae |
| CN107468822A (en) * | 2017-08-16 | 2017-12-15 | 广西克鲁尼茶叶生物科技有限公司 | A kind of resin extraction process of high-purity tea polypenols |
| CN112195063A (en) * | 2020-09-30 | 2021-01-08 | 株洲神农茶油发展有限公司 | Preparation method of tea seed oil rich in tea polyphenol |
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- 2022-05-26 CN CN202210581856.7A patent/CN114854487A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105567420A (en) * | 2015-12-24 | 2016-05-11 | 福建优创油脂有限公司 | Preparation method of health care tea oil |
| CN106190524A (en) * | 2016-08-18 | 2016-12-07 | 贵州石阡佛顶山野生油茶油业有限公司 | A kind of production method of aqueous enzymatic extraction Oleum Camelliae |
| CN107468822A (en) * | 2017-08-16 | 2017-12-15 | 广西克鲁尼茶叶生物科技有限公司 | A kind of resin extraction process of high-purity tea polypenols |
| CN112195063A (en) * | 2020-09-30 | 2021-01-08 | 株洲神农茶油发展有限公司 | Preparation method of tea seed oil rich in tea polyphenol |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115232669A (en) * | 2022-08-11 | 2022-10-25 | 贵州山茶产业综合开发有限公司 | Preparation method of squalene-containing tea oil |
| CN115232669B (en) * | 2022-08-11 | 2024-02-09 | 贵州山茶产业综合开发有限公司 | Preparation method of tea oil containing squalene |
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